EP2011848A1 - Method for stabilising heating oil or diesel oil, particularly from depolymerisation of residue containing hydrocarbons or pyrolisis oil - Google Patents

Method for stabilising heating oil or diesel oil, particularly from depolymerisation of residue containing hydrocarbons or pyrolisis oil Download PDF

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EP2011848A1
EP2011848A1 EP08012226A EP08012226A EP2011848A1 EP 2011848 A1 EP2011848 A1 EP 2011848A1 EP 08012226 A EP08012226 A EP 08012226A EP 08012226 A EP08012226 A EP 08012226A EP 2011848 A1 EP2011848 A1 EP 2011848A1
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Prior art keywords
oil
diesel
heating
pyrolysis
degrees
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German (de)
French (fr)
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EP2011848B1 (en
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Manfred Sappok
Dieter Wagels
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WAGELS, DIETER
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Sappok Manfred
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • C10G1/10—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal from rubber or rubber waste
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G27/00—Refining of hydrocarbon oils in the absence of hydrogen, by oxidation
    • C10G27/04—Refining of hydrocarbon oils in the absence of hydrogen, by oxidation with oxygen or compounds generating oxygen
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
    • C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
    • C10G53/14—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one oxidation step
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G7/00—Distillation of hydrocarbon oils
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
    • C10G2400/04—Diesel oil
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
    • C10G2400/06—Gasoil

Definitions

  • the invention relates to a method having the features of the preamble of claim 1. Thereafter, the invention first relates to a method for stabilizing fuel oil and diesel oil, which, in particular after depolimerizing hydrocarbonaceous residues, was obtained by fractional distillation .. In addition, the method is used to stabilize of pyrolysis oils, so that they can be used after the stabilization process as a fuel in heavy oil-driven units (machines).
  • machines heavy oil-driven units
  • a pyrolysis oil is produced.
  • Pyrolysis is the heating of organic matter under exclusion of oxygen. Delimits the pyrolysis against a thermolysis undertakes M.Krapf in Z. Angew. Chemistry 98, 1986, 413-429 .
  • the pyrolysis process takes place in the case of so-called high-temperature pyrolysis at temperatures between 600 ° C and 800 ° C.
  • the product oil (pyrolysis oil) produced in this way has the same problem as products obtained by depolimerization, because even the pyrolysis oil is darkened by the presence of unsaturated hydrocarbons. In order to make it suitable for use in heavy-duty engines, a further process step is necessary.
  • the object of the invention is to remove the dark coloring of diesel and heating oil, in particular if it has been obtained by depolimerization of hydrocarbon-containing residues, or of pyrolysis oil in a simple way.
  • complex hydrogenation processes should be avoided.
  • the coloring process of the starting oil can largely be prevented or slowed down considerably if the starting oil is stored, for example, under inert gas and / or in the dark in a tank, preferably with the exclusion of air and not too high temperatures.
  • the aging or inking process then proceeds very slowly, or is stopped. If, for example, air is admitted into a base oil tank, it may take several weeks, for example B. take 2 or 3 weeks until a significant change in color occurs. It may therefore be useful to store the fresh produced starting oil accordingly, in order to delay the aging process.
  • an oxidative treatment e.g. performed with air.
  • the dark color can be set in a few seconds.
  • the Enrfärbungsdestillation can be carried out both in a conventional distillation column and in a so-called thin-film evaporator.
  • the discolored starting oil is heated to a temperature between 350 and 390 degrees C, preferably 360 to 380 degrees C, and distilled at about 280 to 320 degrees C, preferably at 290 to 310 degrees C.
  • the discolored starting oil is passed in a thin-layer evaporator, preferably under reduced pressure, over about 180 to 240 ° C., preferably at 200 to 230 ° C. hot evaporator surface, and subsequently the resulting vapor component, in particular as diesel or heating oil condensed.
  • the thin-film evaporation takes place under a pressure of absolutely about 1 to 500 mbar, preferably from 2 to 100 mbar.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The method involves allowing or promoting a dark discoloration of diesel oil, and heating oil or pyrolysis oil. The diesel oil is discolored, and the heating oil or pyrolysis oil is subjected to a distillation step with elimination of the dark color. The heating oil or diesel oil to be stabilized is obtained by fractional distillation of a vapor phase from a process of depolymerization of hydrocarbon-containing residues. The dark discoloration is delayed or checked during an intermediate storage phase before distillation of the heating.

Description

GEBIET DER ERFINDUNGFIELD OF THE INVENTION

Die Erfindung betrifft ein Verfahren mit den Merkmalen des Oberbegriffs von Anspruch 1. Danach betrifft die Erfindung zunächst ein Verfahren zum Stabilisieren von Heizöl und Dieselöl, welches, insbesondere nach Depolimerisieren von kohlenwasserstoffhaltigen Rückständen, durch fraktionierte Destillation gewonnen wurde.. Daneben dient das Verfahren zum Stabilisieren von Pyrolyseölen, so dass diese nach dem Stabilisierungsprozess als Brennstoff in mit Schweröl betriebenen Aggregaten (Maschinen) eingesetzt werden können.The invention relates to a method having the features of the preamble of claim 1. Thereafter, the invention first relates to a method for stabilizing fuel oil and diesel oil, which, in particular after depolimerizing hydrocarbonaceous residues, was obtained by fractional distillation .. In addition, the method is used to stabilize of pyrolysis oils, so that they can be used after the stabilization process as a fuel in heavy oil-driven units (machines).

TECHNOLOGISCHER HINTERGRUNDTECHNOLOGICAL BACKGROUND

Durch Depolimerisation von kohlenwasserstoffhaltigen Rückständen gewonnenes Heiz- und Dieselöl ist aus der DE 10 2005 010 151 B3 bekannt. Die Depolimerisation der kohlenwasserstoffhaltigen Rohmaterialien erfolgt dadurch, dass das Rohmaterial, wie Kunststoff oder Altölm, in einem auf Spalttemperatur beheizten Reaktor in flüssiger oder breiiger Konsistenz in einem vorbeheizten Zustand unter Druck eingespritzt wird. Aus dem indirekt über die Mantelfläche auf z.B. 420°C Innentemperatur beheizten Reaktor wird eine dampfförmige Fraktion abgezogen, aus der durch fraktionierte Destillation auf direktem Wege eine Diesel- oder Heizölfraktion gewonnen wird. Der in dem Reaktor anfallende Feststoff wird kontinuierlich abgezogen und weiterverarbeitet. Es hat sich herausgestellt, dass sich insbesondere bei diesem Gewinnungsverfahren für Heizöl und Dieseöl ein zunächst sehr klares. Produkt ergibt, welches sich allerdings nach einiger Zeit einfärbt, bis es fast schwarz aussieht. Zwar wird dadurch die Verwendbarkeit als Diesel- oder Heizkraftstoff nicht beeinträchtigt, dennoch wird eine solche Färbung des Produktes von den Kunden nicht akzeptiert.By Depolimerisation of hydrocarbon-containing residues obtained heating and diesel oil is from the DE 10 2005 010 151 B3 known. The Depolimerisation of hydrocarbonaceous raw materials takes place in that the raw material, such as plastic or waste oil, in a reactor heated to nip temperature in liquid or pulpy consistency is injected under pressure in a preheated state. From the indirectly heated over the jacket surface, for example, 420 ° C internal temperature reactor, a vapor fraction is withdrawn, from which by fractional distillation directly a diesel or Heizölfraktion is obtained. The solid obtained in the reactor is continuously withdrawn and processed. It has been found that, in particular, in this extraction process for heating oil and diesel oil is initially very clear. Product results, which, however, colors after some time until it looks almost black. Although this does not affect the usability as a diesel fuel or heating fuel, such a coloration of the product is not accepted by the customers.

Bei Motorölen ist eine Viskositätserhöhung die auch mit Dunkelfärbung verbunden sein kann, aufgrund einer so genannten Öloxidation bekannt, für die es allerdings keine Ölbehandlung gibt. Vielmehr wird der Austausch so veränderter Öle propagiert. Bei Motorkraftstoffen, insbesondere wenn sie durch Cracken oder Pyrolyse hergestellt werden, kann die Lagerstabilität durch Zugabe von Antioxidationsmitteln, wie unter dem Markennamen "Kerobit" der Firma BASF bekannt, verbessert werden. Dadurch sollen die von freien Radikalen an den Enden von Kohlenwasserstoffketten begünstigten Polymerisationsreaktionen unterbunden werden. Derartige Additive sind zumeist aber gesundheitsgefährdend.In the case of engine oils, an increase in viscosity, which may also be associated with darkening, is known due to a so-called oil oxidation, for which, however, there is no oil treatment. Rather, the exchange of so changed oils is propagated. In the case of motor fuels, in particular when they are prepared by cracking or pyrolysis, the storage stability can be improved by adding antioxidants, as known under the trade name "Kerobit" from BASF. This is intended to inhibit the polymerization reactions promoted by free radicals at the ends of hydrocarbon chains. Such additives are usually hazardous to health.

Bei der Pyrolyse, insbesondere von Gummi und anderen nachwachsenden Rohstoffen wird ein Pyrolyseöl erzeugt. Unter. Pyrolyse versteht man die Erhitzung von organischen Stoffen unter Sauerstoffabschluss. Eine Abgrenzung der Pyrolyse gegenüber einer Thermolyse unternimmt M.Krapf in Z. Angew. Chemie 98, 1986, 413- 429 . Der Pyrolyseprozess findet im Falle der so genannten Hochtemperaturpyrolyse statt bei Temperaturen zwischen 600°C und 800°C. Das so hergestellte Produktöl (Pyrolyseöl) hat das gleiche Problem wie durch Depolimerisation gewonnene Produkte, denn auch das Pyrolyseöl wird durch das Vorhandensein ungesättigter Kohlenwasserstoffe dunkel verfärbt. Um es für den Einsatz in Schwermotoren tauglich zu machen, ist ein weiterer Verfahrensschritt notwendig.In pyrolysis, especially of rubber and other renewable resources, a pyrolysis oil is produced. Under. Pyrolysis is the heating of organic matter under exclusion of oxygen. Delimits the pyrolysis against a thermolysis undertakes M.Krapf in Z. Angew. Chemistry 98, 1986, 413-429 , The pyrolysis process takes place in the case of so-called high-temperature pyrolysis at temperatures between 600 ° C and 800 ° C. The product oil (pyrolysis oil) produced in this way has the same problem as products obtained by depolimerization, because even the pyrolysis oil is darkened by the presence of unsaturated hydrocarbons. In order to make it suitable for use in heavy-duty engines, a further process step is necessary.

DARSTELLUNG DER ERFINDUNGPRESENTATION OF THE INVENTION

Davon ausgehend liegt der Erfindung die Aufgabe zugrunde, die dunkle Färbung von Diesel- und Heizöl, insbesondere wenn es durch Depolimerisation von kohlenwasserstoffhaltigen Rückständen gewonnen worden ist, oder von Pyrolyseöl auf einfachem Wege zu entfernen. Insbesondere sollen aufwendige Hydrierprozesse vermieden werden. Zur Lösung dieser Aufgabe wird vorgeschlagen, zunächst ein Dunkelfärben des Diesel-, Heiz-oder Pyrolyseöls (nachfolgend gemeinsam auch als Ausgangsöl bezeichnet), insbesondere unter Sauerstoffzutritt, zu gestatten oder zu fördern und nachfolgend das dunkel verfärbte Ausgangsöl einer Destillation bzw. erneuten Destillation (nachfolgend auch als Entfärbungsdestillstion bezeichnet) zu unterziehen. Es wurde festgestellt, dass durch dieses Verfahren ein helles und klares Produkt ohne Trübung entsteht und dieses Produkt auch langfristig klar und hell bleibt. Auf diese Weise konnten Eigenschaftswerte eines Dieselkraftstoffes nach DIN EN 590 und Eigenschaftswerte für Heizöl nach DIN 51603/1 erreicht werden, jedenfalls soweit der enthaltene Schwefel auf entsprechende Grenzen reduziert wurde.Based on this, the object of the invention is to remove the dark coloring of diesel and heating oil, in particular if it has been obtained by depolimerization of hydrocarbon-containing residues, or of pyrolysis oil in a simple way. In particular, complex hydrogenation processes should be avoided. To solve this problem, it is proposed to first allow darkening of the diesel, heating or pyrolysis oil (hereinafter also referred to as the starting oil), in particular under oxygen access, and subsequently to transport the darkly colored starting oil to a distillation or redistillation (hereafter also referred to as Entfärbungsdestillstion) to undergo. It has been found that this process produces a bright and clear product without turbidity and keeps this product clear and bright in the long term. In this way, property values of a diesel fuel in accordance with DIN EN 590 and property values for heating oil in accordance with DIN 51603/1 could be achieved, at least insofar as the sulfur contained was reduced to corresponding limits.

Der Einfärbprozess des Ausgangsöls kann weitgehend unterbunden oder sehr stark verlangsamt werden, wenn das Ausgangsöl z.B. unter Schutzgas und/oder bei Dunkelheit in einem Tank, vorzugsweise unter Ausschluss von Luftzutritt und bei nicht zu hohen Temperaturen gelagert wird. Der Alterungs- oder Einfärbprozess schreitet dann nur äußerst langsam voran, oder wird gestoppt. Gestattet man z.B. Luftzutritt in einen Ausgangsöltank, so kann es einige Wochen z. B. 2 oder 3 Wochen dauern, bis eine deutliche Farbveränderung eintritt. Es kann also sinnvoll sein, das frische hergestellte Ausgangsöl entsprechend zu lagern, um den Alterungsprozess hinauszuzögern.The coloring process of the starting oil can largely be prevented or slowed down considerably if the starting oil is stored, for example, under inert gas and / or in the dark in a tank, preferably with the exclusion of air and not too high temperatures. The aging or inking process then proceeds very slowly, or is stopped. If, for example, air is admitted into a base oil tank, it may take several weeks, for example B. take 2 or 3 weeks until a significant change in color occurs. It may therefore be useful to store the fresh produced starting oil accordingly, in order to delay the aging process.

Um die erfindungsgemäße Behandlung des Ausgangsöls zu beschleunigen, wird eine oxidative Behandlung, z.B. mit Luft durchgeführt. Wenn man das Ausgangsöl z.B. sprudelnd mit Luft durchströmt, kann sich die Dunkelfärbung in wenigen Sekunden einstellen.To accelerate the treatment of the starting oil according to the invention, an oxidative treatment, e.g. performed with air. When the starting oil is e.g. bubbly flows through with air, the dark color can be set in a few seconds.

Die Enrfärbungsdestillation kann sowohl in einer üblichen Destillationskolonne als auch in einem so genannten Dünnschichtverdampfer durchgeführt werden. Bei der Enrfärbungsdestillation wird das verfärbte Ausgangsöl auf eine Temperatur zwischen 350 und 390 Grad C, vorzugsweise auf 360 bis 380 Grad C, aufgeheizt und bei etwa 280 bis 320 Grad C, vorzugsweise bei 290 bis 310 Grad C destilliert. Bei der Dünnschichtverdampfung wird das verfärbte Ausgangsöl in einem, vorzugsweise auf Unterdruck gehaltenen, Dünnschichtverdampfer als Dünnschicht über eine etwa 180 bis 240 Grad C, vorzugsweise bei 200 bis 230 Grad C heiße Verdampferfläche geleitet und nachfolgend die dabei dampfförmig anfallende Komponente insbesondere als Diesel- oder Heizöl kondensiert. Die Dünnschichtverdampfung erfolgt unter einem Druck von absolut etwa 1 bis 500 mbar, vorzugsweise von 2 bis 100 mbar.The Enrfärbungsdestillation can be carried out both in a conventional distillation column and in a so-called thin-film evaporator. In the dyeing distillation, the discolored starting oil is heated to a temperature between 350 and 390 degrees C, preferably 360 to 380 degrees C, and distilled at about 280 to 320 degrees C, preferably at 290 to 310 degrees C. In the case of thin-film evaporation, the discolored starting oil is passed in a thin-layer evaporator, preferably under reduced pressure, over about 180 to 240 ° C., preferably at 200 to 230 ° C. hot evaporator surface, and subsequently the resulting vapor component, in particular as diesel or heating oil condensed. The thin-film evaporation takes place under a pressure of absolutely about 1 to 500 mbar, preferably from 2 to 100 mbar.

Durch die Erfindung können, u. a., unerwartet hohe Anteile des verfärbten Ausgangsöls als dauerhaft klares Produkt erzielt werden.By the invention, u. a., Unexpectedly high levels of discolored starting oil are achieved as a permanently clear product.

Die gleiche Verfahrensweise bei den gleichen Prozessparametern kann man also sowohl bei der Entfärbung von Diesel- oder Heizöl als auch bei der Entfärbung bzw. Reinigung von Pyrolyseöl anwenden, auch bei Letzterer wird eine Klarfärbung des Pyrolyseöls erzielt und das somit hergestellte Nutzprodukt ist verwertbar in Verbrennungsmotoren. Es bleibt dauerhaft klar.The same procedure with the same process parameters can thus be used both in the decolorization of diesel or heating oil and in the decolorization or purification of pyrolysis oil, even in the latter a clear coloration of the pyrolysis oil is achieved and the useful product thus produced is usable in internal combustion engines. It stays clear for a long time.

Die vorgenannten sowie die beanspruchten und in den Ausführungsbeispielen beschriebenen erfindungsgemäß zu verwendenden Bauteile unterliegen in ihrer Größe, Formgestaltung, Materialauswahl und technischen Konzeption sowie den übrigen Verfahrensbedingungen keinen besonderen Ausnahmebedingungen, so dass die in dem Anwendungsgebiet bekannten Auswahlkriterien uneingeschränkt Anwendung finden könnenThe abovementioned and the claimed components to be used according to the invention described in the exemplary embodiments are not subject to any special conditions of exception in terms of their size, shape design, material selection and technical conception as well as the other process conditions, so that the details given in US Pat Application field known selection criteria can fully apply

Weitere Einzelheiten, Merkmale und Vorteile des Gegenstandes der Erfindung ergeben sich aus den Unteransprüchen, sowie aus der nachfolgenden Beschreibung eines Ausführungsbeispiels für durch Depolymerisation gewonnenes Heizöl mit anschließender Bidestillation durch Dünnschichtverdampfung.Further details, features and advantages of the subject matter of the invention will become apparent from the dependent claims, as well as from the following description of an embodiment of recovered by depolymerization heating oil with subsequent bid distillation by thin film evaporation.

AUSFÜHRUNGSBEISPIELEmbodiment

Ein gemäß DE 10 2005 010 151 B3 aus Altöl gewonnenes verfärbtes Heizöl wurde in einem VDL 70 Dünnschichtverdampfer mit 4dm2 - WRS auf 210 Grad C bei 5,2 mbar verdampft. Dabei fiel ein flüssiger Rückstand von 4,5% und ein Kondensationsverlust von 1,0% an. 94.5% fielen als dauerhaft klares Bidestillat an. Durch eine Erhöhung der Verdampfertemperatur auf 220 Grad C wurde der Flüssigrückstand auf 1,1 % gesenkt, und es fielen 97,9% als dauerhaft klares Bidestillat an.One according to DE 10 2005 010 151 B3 discolored fuel oil obtained from waste oil was evaporated in a VDL 70 thin film evaporator with 4dm 2 WRS to 210 ° C at 5.2 mbar. This resulted in a liquid residue of 4.5% and a condensation loss of 1.0%. 94.5% was a permanently clear distillate. Increasing the evaporator temperature to 220 degrees C lowered the liquid residue to 1.1 percent and 97.9 percent was a consistently clear distillate distillate.

Claims (9)

Verfahren zum Stabilisieren von Heizöl und Dieselöl welches durch fraktionierte Destillation gewonnen wurde oder von Pyrolyseöl, das bei der Pyrolyse von Gummi oder organischen Stoffen gewonnen wurde, dadurch gekennzeichnet, dass zunächst ein Dunkelfärben des Dieselöls, des Heizöls oder des Pyrolyseöls gestattet oder gefördert wird und nachfolgend das dunkel verfärbte Dieselöl, Heizöl oder Pyrolyseöl einem Destillationsschritt unter Befreiung von der Dunkelverfärbung unterzogen wird.Process for stabilizing fuel oil and diesel oil obtained by fractional distillation or from pyrolysis oil obtained in the pyrolysis of rubber or organic substances, characterized in that first darkening of the diesel oil, heating oil or pyrolysis oil is allowed or promoted and subsequently the dark discolored diesel oil, fuel oil or pyrolysis oil is subjected to a distillation step free from dark discoloration. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass das zu stabilisierende Heizöl oder Dieselöl durch fraktionierte Destillation der Dampfphase aus einem Depolimerisierungsprozess von kohlenwasserstoffhaltigen Rückständen gewonnen wurde. ,A method according to claim 1, characterized in that the fuel oil or diesel oil to be stabilized was obtained by fractional distillation of the vapor phase from a Depolimerisierungsprozess of hydrocarbon-containing residues. . Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die Dunkelfärbung während einer Zwischenlagerungsphase vor dem die Dunkelverfärbung entfernenden Destillieren des Heiz-, Diesel- oder Pyrolyseöls durch Verhinderung von Licht- und/oder Luftzutritt oder durch Lagerung unter Schutzgasatmophäre verlangsamt oder gestoppt wird.A method according to claim 1 or 2, characterized in that the darkening is slowed or stopped during an intermediate storage phase before distilling off the dark discoloration of the heating, diesel or pyrolysis oil by preventing light and / or air access or storage under inert gas atmosphere. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass vor den die Dunkelverfärbung entfernenden Destillieren eine Behandlung des Heiz-, Diesel- oder Pyrolyseöls unter oxidativer Atmosphäre, insbesondere mit Sauerstoff, erfolgt.Method according to one of claims 1 to 3, characterized in that prior to removing the dark discoloration distilling a treatment of the heating, diesel or pyrolysis oil under oxidative atmosphere, in particular with oxygen. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass während der Dunkelfärbphase das Heiz-, Diesel- oder Pyrolyseöl einer intensiven Durchmischung, wie, vorzugsweise, einer Durchsprudelung, mit mindestens einem oxidativ wirkenden Fluid unterzogen wird.Method according to one of claims 1 to 4, characterized in that during the dark-colored phase, the heating, diesel or pyrolysis oil is subjected to intensive mixing, such as, preferably, a bubbling, with at least one oxidatively acting fluid. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass die die Dunkelverfärbung entfernende Destillation in einer Destillationskolonne oder in einem Dünnschichtverdampfer durchgeführt wird.Method according to one of claims 1 to 5, characterized in that the removing the dark discoloration distillation is carried out in a distillation column or in a thin-film evaporator. Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, dass das verfärbte Heiz-, Diesel- oder Pyrolyseöl auf eine Temperatur zwischen 350 und 390 Grad C, vorzugsweise auf 360 bis 380 Grad C, aufgeheizt und bei etwa 280 bis 320 Grad C, vorzugsweise bei 290 bis 310 Grad C destilliert wird.Method according to one of claims 1 to 6, characterized in that the discolored heating, diesel or pyrolysis oil to a temperature between 350 and 390 degrees C, preferably at 360 to 380 degrees C, heated and at about 280 to 320 degrees C, preferably distilled at 290 to 310 degrees C. Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, dass das verfärbte Heiz-, Diesel- oder Pyrolyseöl in einem, vorzugsweise auf Unterdruck gehaltenen, Dünnschichtverdampfer als Dünnschicht über eine etwa 180 bis 240 Grad C, vorzugsweise bei 200 bis 230 Grad C heiße Verdampferfläche geleitet und nachfolgend die dabei dampfförmig anfallende Komponente als Diesel-, Heiz- oderSchweröl kondensiert wird.Method according to one of claims 1 to 6, characterized in that the discolored heating, diesel or pyrolysis oil in a, preferably held on vacuum, thin-film evaporator as a thin layer over about 180 to 240 degrees C, preferably 200 to 230 degrees C hot Evaporator surface passed and then the resulting vapor component is condensed as diesel, heating or heavy oil. Verfahren nach Anspruch 8, dadurch gekennzeichnet, dass die Dünnschichtverdampfung unter einem Druck von absolut etwa 1 bis 500 mbar, vorzugsweise von 2 bis 100 mbar erfolgt.A method according to claim 8, characterized in that the thin-film evaporation under a pressure of absolutely about 1 to 500 mbar, preferably from 2 to 100 mbar.
EP08012226.0A 2007-07-05 2008-07-07 Method for stabilising heating oil or diesel oil, particularly from depolymerisation of residue containing hydrocarbons, or pyrolysis oil Active EP2011848B1 (en)

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US8394264B2 (en) 2013-03-12
CA2636956A1 (en) 2009-01-05
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